CN107381626A - A kind of iron content layered potassium titanate platy particles and its hydrothermal preparing process - Google Patents
A kind of iron content layered potassium titanate platy particles and its hydrothermal preparing process Download PDFInfo
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- CN107381626A CN107381626A CN201710743855.7A CN201710743855A CN107381626A CN 107381626 A CN107381626 A CN 107381626A CN 201710743855 A CN201710743855 A CN 201710743855A CN 107381626 A CN107381626 A CN 107381626A
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- potassium titanate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/005—Alkali titanates
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
Abstract
The invention discloses a kind of iron content layered potassium titanate platy particles and preparation method thereof, belong to field of material preparation.By TiO2With Fe (NO3)3·9H2O is added in the KOH aqueous solution, and stirring is well mixed raw material, carries out hydro-thermal reaction, after reaction terminates, filtered, washing, is dried, is obtained iron content layered potassium titanate platy particles.The composition expression formula of the platy particles is K0.8Fe0.8Ti1.2O4, its length is 1~2 μm, and thickness is 100~200nm.The stratiform K prepared compared to conventional solid-state method and molten-salt growth method, the technology of the present invention0.8Fe0.8Ti1.2O4Platy particles particle diameter is small, purity is high, pattern and microstructure are controllable, and its preparation technology is simple, and energy consumption is low, and repeatability is high, is advantageous to industrialized production.
Description
Technical field
The invention belongs to field of material preparation, and in particular to prepared by a kind of iron content layered potassium titanate platy particles and its hydro-thermal
Method.
Background technology
Layered titanate is a kind of typical lamellar compound, and there is good photocatalytic, electrochemistry and ion to hand over
It is transsexual to wait, and can by doping, interlayer is pillared etc., and modification means carry out the design of molecular level to it, cut out and assemble,
The photocatalytic activity and chemical property of material are improved, there is important potential using value.
Layered titanate is as battery active material and catalysis material, and its performance is largely by its microcosmic shape
Looks, particle diameter and specific surface area are determined.At present, iron content layered potassium titanate (K0.8Fe0.8Ti1.2O4) preparation method be mainly
Solid phase method and molten-salt growth method.Minoru Osada et al. [Advanced Materials, 2006,18 (3):295-299.] by solid
Phase reaction method, by K2CO3, TiO2And Fe2O3Uniformly mixed with certain mol ratio, 24h is reacted under 1100 DEG C of high temperature and is prepared
The K of stratiform0.8Fe0.8Ti1.2O4；Fengxia Geng, Takayoshi Sasaki et al. [Journal of the American
Chemical Society,2014,136(14):5491-5500.] by TiO2, Fe2O3, K2CO3And MoO3Mixing, add excessive
K2CO3Make a part of K2CO3As reaction raw materials, another part K2CO3With MoO3Reaction generation K at high temperature2MoO4, with
K2MoO4For fused salt, synthesize the K of stratiform under high temperature by molten-salt growth method0.8Fe0.8Ti1.2O4.The stratiform that these methods are prepared
K0.8Fe0.8Ti1.2O4With particle diameter is big, particle diameter distribution wide (length is about 5~50 μm, and thickness is 2~5 μm) and purity are low.This
Outside, all there is complex process in these methods, high energy consumption, the shortcomings of reaction time is long, be unfavorable for industrialized production.
The content of the invention
The defects of in order to overcome above-mentioned prior art to exist, it is an object of the invention to provide a kind of iron content layered potassium titanate
Platy particles and its hydrothermal preparing process, this method reaction condition is gentle, simple to operate, and repeatability is high, by containing for party's legal system
The particle diameter of iron layered potassium titanate particle is small, purity is high, pattern and microstructure are controllable.
To achieve these goals, the present invention uses following technical scheme.
The hydrothermal preparing process of a kind of iron content layered potassium titanate platy particles disclosed by the invention, by TiO2And Fe
(NO3)3·9H2O is added in the KOH aqueous solution, and stirring is well mixed raw material, carries out hydro-thermal reaction, after reaction terminates, is passed through
Filter, washing, dry, obtain iron content layered potassium titanate platy particles.
Preferably, the TiO2、Fe(NO3)3·9H2The amount ratio of the O and KOH aqueous solution is 5g：16.87g：(15~100)
mL。
Preferably, the mass concentration of the described KOH aqueous solution is 3~10mol/L.
Preferably, described hydrothermal temperature is 150~300 DEG C.
Preferably, described the hydro-thermal reaction time is 4~24h.
Preferably, the washing is carried out using water, and drying is carried out at 50~80 DEG C.
The invention also discloses using iron content layered potassium titanate platy particles made from above-mentioned hydrothermal preparing process, this contains
The composition expression formula of iron layered potassium titanate platy particles is K0.8Fe0.8Ti1.2O4。
Preferably, the length of the iron content layered potassium titanate platy particles is 1~2 μm, and thickness is 100~200nm.
Compared with prior art, the invention has the characteristics that：
The hydrothermal preparing process of iron content layered potassium titanate platy particles disclosed by the invention, with TiO2As titanium source, Fe
(NO3)3·9H2O is sufficiently mixed as source of iron, and with the certain density KOH aqueous solution, carries out hydrothermal crystallization reaction, and iron content is made
The K of layer structure0.8Fe0.8Ti1.2O4Platy particles, its particle diameter is small and narrowly distributing (length is about 1~2 μm, thickness is 100~
200nm)；Compared to conventional solid-state method and molten-salt growth method, preparation technology of the invention is simple, and energy consumption is low, and repeatability is high, is advantageous to industry
Metaplasia is produced.
Further, hydro-thermal reaction of the invention is carried out at 150~300 DEG C, and treatment temperature is relatively low, compared to existing skill
Need to carry out at 1100 DEG C in art, hence it is evident that there is the advantage that energy consumption is low, equipment requirement is low, environment-friendly.
The stratiform K prepared through inventive method0.8Fe0.8Ti1.2O4Platy particles particle diameter is small, purity is high, pattern and microstructure
It is controllable.
Brief description of the drawings
Fig. 1 is the XRD spectrum of iron content layered potassium titanate particle prepared by the present invention；
Fig. 2 is the SEM photograph of iron content layered potassium titanate particle prepared by the present invention.
Embodiment
Below in conjunction with the accompanying drawings and specific embodiment is described in further detail to the present invention：
Embodiment 1
By 5g TiO2With 16.87g Fe (NO3)3·9H2O is added in the KOH aqueous solution that 15mL concentration is 3mol/L, is stirred
Mixing is well mixed raw material, and hydro-thermal reaction 4h is carried out at 150 DEG C, after reaction terminates, filtered, washing, dries, obtains containing iron layer
Shape potassium titanate K0.8Fe0.8Ti1.2O4Platy particles, its length are about 1~2 μm, and thickness is 100~200nm.
Embodiment 2
By 5g TiO2With 16.87g Fe (NO3)3·9H2O is added in the KOH aqueous solution that 20mL concentration is 6mol/L, is stirred
Mixing is well mixed raw material, and hydro-thermal reaction 8h is carried out at 180 DEG C, after reaction terminates, filtered, washing, dries, obtains containing iron layer
Shape potassium titanate K0.8Fe0.8Ti1.2O4Platy particles, its length are about 1~2 μm, and thickness is 100~200nm.
Embodiment 3
By 5g TiO2With 16.87g Fe (NO3)3·9H2O is added in the KOH aqueous solution that 15mL concentration is 10mol/L,
Stirring is well mixed raw material, and hydro-thermal reaction 12h is carried out at 250 DEG C, after reaction terminates, filtered, washing, dries, is contained
Iron layered potassium titanate K0.8Fe0.8Ti1.2O4Platy particles, its length are about 1~2 μm, and thickness is 100~200nm.
Embodiment 4
By 5g TiO2With 16.87g Fe (NO3)3·9H2O is added in the KOH aqueous solution that 50mL concentration is 10mol/L,
Stirring is well mixed raw material, and hydro-thermal reaction 12h is carried out at 280 DEG C, after reaction terminates, filtered, washing, dries, is contained
Iron layered potassium titanate K0.8Fe0.8Ti1.2O4Platy particles, its length are about 1~2 μm, and thickness is 100~200nm.
Embodiment 5
By 5g TiO2With 16.87g Fe (NO3)3·9H2O is added in the KOH aqueous solution that 50mL concentration is 10mol/L,
Stirring is well mixed raw material, and hydro-thermal reaction 24h is carried out at 300 DEG C, after reaction terminates, filtered, washing, dries, is contained
Iron layered potassium titanate K0.8Fe0.8Ti1.2O4Platy particles, its length are about 1~2 μm, and thickness is 100~200nm.
Embodiment 6
By 5g TiO2With 16.87g Fe (NO3)3·9H2O is added in the KOH aqueous solution that 70mL concentration is 6mol/L, is stirred
Mixing is well mixed raw material, and hydro-thermal reaction 15h is carried out at 200 DEG C, after reaction terminates, filtered, washing, dries, obtains iron content
Layered potassium titanate K0.8Fe0.8Ti1.2O4Platy particles, its length are about 1~2 μm, and thickness is 100~200nm.
Embodiment 7
By 5g TiO2With 16.87g Fe (NO3)3·9H2O is added in the KOH aqueous solution that 45mL concentration is 3mol/L, is stirred
Mixing is well mixed raw material, and hydro-thermal reaction 24h is carried out at 150 DEG C, after reaction terminates, filtered, washing, dries, obtains iron content
Layered potassium titanate K0.8Fe0.8Ti1.2O4Platy particles, its length are about 1~2 μm, and thickness is 100~200nm.
Embodiment 8
By 5g TiO2With 16.87g Fe (NO3)3·9H2O is added in the KOH aqueous solution that 100mL concentration is 3mol/L,
Stirring is well mixed raw material, and hydro-thermal reaction 4h is carried out at 300 DEG C, after reaction terminates, filtered, washing, dries, obtains iron content
Layered potassium titanate K0.8Fe0.8Ti1.2O4Platy particles, its length are about 1~2 μm, and thickness is 100~200nm.
It is the iron content layered potassium titanate K prepared by the present invention referring to Fig. 10.8Fe0.8Ti1.2O4The XRD spectrum of platy particles.
As seen from the figure, iron content layered potassium titanate K obtained by the present invention0.8Fe0.8Ti1.2O4Platy particles are 10 degree attached in 2theta
Closely show layered titanate characteristic diffraction peak.
Table 1 is to be analyzed to obtain the chemical group of present invention preparation cobalt containing layer shape potassium titanate platy particles by X-ray fluorescence spectra
Into the chemical composition that the present invention prepares cobalt containing layer shape potassium titanate platy particles as can be seen from Table 1 is K0.8Zn0.4Ti1.6O4。
The element composition for the particle of layered potassium titanate containing zinc that table 1 is prepared for the present invention
| Composition | K2O | ZnO | TiO2 |
| Molar percentage (%) | 17.24 | 16.12 | 66.64 |
Referring to Fig. 2, it is the iron content layered potassium titanate K prepared by the present invention0.8Fe0.8Ti1.2O4The SEM of platy particles shines
Piece.It can be clearly seen that from figure：The iron content layered potassium titanate K that the present invention obtains0.8Fe0.8Ti1.2O4Platy particles pattern is
Tabular, its length are about 1~2 μm, and thickness is 100~200nm.
Claims (8)
1. a kind of hydrothermal preparing process of iron content layered potassium titanate platy particles, it is characterised in that by TiO2With Fe (NO3)3·
9H2O is added in the KOH aqueous solution, and stirring is well mixed raw material, carries out hydro-thermal reaction, after reaction terminates, filtered, washing,
Dry, obtain iron content layered potassium titanate platy particles.
2. the hydrothermal preparing process of iron content layered potassium titanate platy particles according to claim 1, it is characterised in that：It is described
TiO2、Fe(NO3)3·9H2The amount ratio of the O and KOH aqueous solution is 5g：16.87g：(15~100) mL.
A kind of 3. hydrothermal preparing process of iron content layered potassium titanate platy particles according to claim 1, it is characterised in that：
The mass concentration of the described KOH aqueous solution is 3~10mol/L.
A kind of 4. hydrothermal preparing process of iron content layered potassium titanate platy particles according to claim 1, it is characterised in that：
Described hydrothermal temperature is 150~300 DEG C.
A kind of 5. hydrothermal preparing process of iron content layered potassium titanate platy particles according to claim 1, it is characterised in that：
Described the hydro-thermal reaction time is 4~24h.
A kind of 6. hydrothermal preparing process of iron content layered potassium titanate platy particles according to claim 1, it is characterised in that：
The washing is carried out using water, and drying is carried out at 50~80 DEG C.
7. using iron content layered potassium titanate tabular grain made from the hydrothermal preparing process described in any one in claim 1~6
Son, it is characterised in that：The composition expression formula of the iron content layered potassium titanate platy particles is K0.8Fe0.8Ti1.2O4。
8. iron content layered potassium titanate platy particles according to claim 7, it is characterised in that：The iron content layered potassium titanate plate
The length of shape particle is 1~2 μm, and thickness is 100~200nm.
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